CN103272575B - A kind of nanometer titanic oxide composite photochemical catalyst material and preparation method thereof - Google Patents
A kind of nanometer titanic oxide composite photochemical catalyst material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 35
- 239000003054 catalyst Substances 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 43
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012065 filter cake Substances 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 238000000746 purification Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 8
- 239000011707 mineral Substances 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 230000018044 dehydration Effects 0.000 claims abstract description 7
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 7
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims abstract description 7
- 239000007787 solid Substances 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 20
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 18
- 239000011259 mixed solution Substances 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 150000002500 ions Chemical class 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 6
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 6
- 125000004122 cyclic group Chemical group 0.000 claims description 6
- DCKVFVYPWDKYDN-UHFFFAOYSA-L oxygen(2-);titanium(4+);sulfate Chemical compound [O-2].[Ti+4].[O-]S([O-])(=O)=O DCKVFVYPWDKYDN-UHFFFAOYSA-L 0.000 claims description 6
- 230000003068 static effect Effects 0.000 claims description 6
- 229910000348 titanium sulfate Inorganic materials 0.000 claims description 6
- 239000004113 Sepiolite Substances 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 claims description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052624 sepiolite Inorganic materials 0.000 claims description 2
- 235000019355 sepiolite Nutrition 0.000 claims description 2
- 239000010457 zeolite Substances 0.000 claims description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 47
- 238000000034 method Methods 0.000 abstract description 20
- 230000015556 catabolic process Effects 0.000 abstract description 17
- 238000006731 degradation reaction Methods 0.000 abstract description 17
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 6
- 229940043267 rhodamine b Drugs 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 229910052755 nonmetal Inorganic materials 0.000 abstract description 3
- 229930040373 Paraformaldehyde Natural products 0.000 abstract description 2
- 239000003973 paint Substances 0.000 abstract description 2
- 229920002866 paraformaldehyde Polymers 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 27
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 4
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000005495 cold plasma Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000205 computational method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229910052613 tourmaline Inorganic materials 0.000 description 1
- 229940070527 tourmaline Drugs 0.000 description 1
- 239000011032 tourmaline Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Abstract
A kind of nanometer titanic oxide composite photochemical catalyst material and preparation method thereof, puts into dispersion tank and stirs, filters rear obtained filter cake by nonmetal for natural micropore structure raw ore mineral powder 1 part, 10 parts, water and calgon 0.006 part; The sulfuric acid solution being 30% by gained filter cake and volumetric concentration adds in purification tank and stirs, and obtains suspension; Filtration washing is carried out to gained suspension, obtains carrier; Be that prepared carrier and water join in reactor by 1:25 by quality solid-to-liquid ratio, after stirring, adjust pH value, insulation, obtain mixture; Namely nanometer titanic oxide composite photochemical catalyst material is obtained after gained mixture is carried out filtering means dehydration, washing, drying, cooling; The inventive method is simple, easy, prepared nanometer titanic oxide composite photochemical catalyst material has higher activity, to the harmful substance in air, there is higher degradation rate, the degradation rate of PARA FORMALDEHYDE PRILLS(91,95) can reach more than 80%, in 30min, under uviol lamp, rhodamine B degradation rate can reach 96.41%, can be applicable to the preparation of water paint, has good environment-friendly function.
Description
Technical field
The present invention relates to a kind of catalysis material, is a kind of nanometer titanic oxide composite photochemical catalyst material and preparation method thereof specifically.
Background technology
Indoor formaldehyde, toluene concentration endanger larger pollution in indoor pollution, and serious harm people's is healthy.Because current technological means and material limit, also cannot remove the harm of formaldehyde and toluene in a short time from source, therefore, effectively remove formaldehyde, the toluene concentration in room and office, most important to protection human health.
At present, the administering method of domestic and international formaldehyde and toluene gas mainly contains physisorphtion, chemical reaction method, catalytic oxidation, bioanalysis, composite algorithm and cold plasma method.There is the problem of adsorption equilibrium in physisorphtion, physisorphtion often combines with chemical reaction method by researcher, and based on chemical reaction, physical absorption is auxiliary, can reach good effect like this.Although chemical reaction method can remove rapidly formaldehyde in air and toluene, the method needs to consume a large amount of chemical reagent, and cost is high, and the reagent that some method uses has certain toxicity.In addition also there is the reaction problems such as saturated rear carrier not easily reclaims, waste of material amount is large in chemical reaction method.Heat catalytic oxidation method does not need to consume chemical reagent, does not react saturated problem yet, but often needs higher temperature, be not suitable in indoor use.Photocatalytic method and cold plasma method are the new methods of decomposing formaldehyde and the toluene occurred in the last few years, and cold plasma method resolving time compared with photocatalytic method is short, and disposal ability is large, and decomposition efficiency is high, but the comparatively large (5 ~ 20Wm of consumed energy
-2), and the simple shortcoming using this technology to there is new pollutant such as generation a large amount of nitrogen oxide and multiple hydroxyl radical gas etc.Photocatalysis technology have at room temperature can use, the advantage such as energy consumption is low, non-secondary pollution, be considered to the air purifying process having larger application prospect, but there is catalyst dispersity difference, be difficult to problems such as reclaiming, production cost is high.
Summary of the invention
The deficiency that the present invention is directed to the problems referred to above provides a kind of nanometer titanic oxide composite photochemical catalyst material and preparation method thereof, the method is simple, prepared nanometer titanic oxide composite photochemical catalyst material can effectively degradation of formaldehyde and toluene gas, has good environment-friendly function.
A preparation method for nanometer titanic oxide composite photochemical catalyst material, concrete operation step is as follows:
Step one, get the nonmetal raw ore mineral powder of natural micropore structure 1 part, 10 parts, water and the calgon 0.006 part that meso-position radius is less than 9 microns and put into dispersion tank, 4 minutes are stirred with the rotating speed of 2500r/min, after static 10 minutes, the dispersion liquid getting top filters, solid matter after filtration, is filter cake;
Step 2, by quality solid-to-liquid ratio 1:3.5, the sulfuric acid solution being 30% by gained filter cake in above-mentioned steps one and volumetric concentration adds in purification tank, stirs 40 minutes, obtains suspension;
Step 3, gained suspension in above-mentioned steps two is carried out filtration washing, wash to sulfate radical-free ion, moisture is 50%, and gained solid matter is called purification filter cake, is namely carrier, for subsequent use;
Step 4, be 1:25 by quality solid-to-liquid ratio, add in reactor by the carrier prepared by above-mentioned steps three and water, after stirring 8 minutes with the rotating speed of 600r/min, to add volumetric concentration be the pH value of the sulfuric acid solution adjustment mixed solution of 35% is 1 ~ 3; Then stir with the rotating speed of 500r/min and within 10 minutes, add titanium sulfate aqueous solution that concentration is 3mol/L or the aqueous solution of titanyle sulfate that concentration is 3mol/L in backward mixed solution, its addition is 0.05% of mixed liquor volume; Continue to stir with the rotating speed of 600r/min to add the ammonium sulfate solution that concentration is 200g/L in backward mixed solution in 12 minutes, its addition is 0.03% of mixed liquor volume; Add after stirring 15 minutes with the rotating speed of 600r/min again mass concentration be the ammoniacal liquor adjustment ph value of mixture of 15% for 4.5, then continue to stir with the rotating speed of 600r/min and obtain mixture after being incubated 40 minutes;
Step 5, the mixture obtained by above-mentioned steps four is carried out filtering means dehydration, cyclic washing, to sulfate radical-free ion, obtains solid matter, and gained solid matter is dry 4 little of Powdered at 105 DEG C;
Step 6, above-mentioned steps five gained powdered solid substance to be calcined 4 hours at 660 DEG C ~ 720 DEG C, after cooling of coming out of the stove, namely obtain nanometer titanic oxide composite photochemical catalyst material.
Beneficial effect
A kind of nanometer titanic oxide composite photochemical catalyst material of the present invention and preparation method thereof, preparation method is simple, and prepared nanometer titanic oxide composite photochemical catalyst material can effectively degradation of formaldehyde and other harmful substances; The degradation rate of PARA FORMALDEHYDE PRILLS(91,95) can reach more than 80%; In 30min, under uviol lamp, rhodamine B degradation rate can reach 96.41%, shows that the nanometer titanic oxide composite photochemical catalyst material prepared by the present invention has higher activity, has higher degradation rate, have good application prospect to the harmful substance in air; Can by the preparation of this materials application in water paint, prepared coating can effectively degradation of formaldehyde, toluene and other pernicious gases, have good environment-friendly function.
Detailed description of the invention
A kind of nanometer titanic oxide composite photochemical catalyst material and preparation method thereof, the method is simple, and prepared nanometer titanic oxide composite photochemical catalyst material can effectively degradation of formaldehyde and toluene gas, has good environment-friendly function.
A preparation method for nanometer titanic oxide composite photochemical catalyst material, concrete operation step is as follows:
Step one, get the nonmetal raw ore mineral powder of natural micropore structure 1 part, 10 parts, water and the calgon 0.006 part that meso-position radius is less than 9 microns and put into dispersion tank, 4 minutes are stirred with the rotating speed of 2500r/min, after static 10 minutes, the dispersion liquid getting top filters, solid matter after filtration, is filter cake;
Step 2, by quality solid-to-liquid ratio 1:3.5, the sulfuric acid solution being 30% by gained filter cake in above-mentioned steps one and volumetric concentration adds in purification tank, stirs 40 minutes, obtains suspension;
Step 3, gained suspension in above-mentioned steps two is carried out filtration washing, wash to sulfate radical-free ion, moisture is 50%, and gained solid matter is called purification filter cake, is namely carrier, for subsequent use;
Step 4, be 1:25 by quality solid-to-liquid ratio, add in reactor by the carrier prepared by above-mentioned steps three and water, after stirring 8 minutes with the rotating speed of 600r/min, to add volumetric concentration be the pH value of the sulfuric acid solution adjustment mixed solution of 35% is 1 ~ 3; Then stir with the rotating speed of 500r/min and within 10 minutes, add titanium sulfate aqueous solution that concentration is 3mol/L or the aqueous solution of titanyle sulfate that concentration is 3mol/L in backward mixed solution, its addition is 0.05% of mixed liquor volume; Continue to stir with the rotating speed of 600r/min to add the ammonium sulfate solution that concentration is 200g/L in backward mixed solution in 12 minutes, its addition is 0.03% of mixed liquor volume; Add after stirring 15 minutes with the rotating speed of 600r/min again mass concentration be the ammoniacal liquor adjustment ph value of mixture of 15% for 4.5, then continue to stir with the rotating speed of 600r/min and obtain mixture after being incubated 40 minutes;
Step 5, the mixture obtained by above-mentioned steps four is carried out filtering means dehydration, cyclic washing, to sulfate radical-free ion, obtains solid matter, and gained solid matter is dry 4 little of Powdered at 105 DEG C;
Step 6, above-mentioned steps five gained powdered solid substance to be calcined 4 hours at 660 DEG C ~ 720 DEG C, after cooling of coming out of the stove, namely obtain nanometer titanic oxide composite photochemical catalyst material.
Following examples are used for further illustrating a kind of nanometer titanic oxide composite photochemical catalyst material of the present invention and preparation method thereof, do not have any restriction to the present invention; In invention use raw material all can commercially obtain.
embodiment 1
A preparation method for nanometer titanic oxide composite photochemical catalyst material, concrete operation step is as follows:
Step one, get natural mineral tourmaline powder 1 part, 10 parts, water and the calgon 0.006 part that meso-position radius is less than 9 microns and put into dispersion tank, stir 4 minutes with the rotating speed of 2500r/min, after static 10 minutes, the dispersion liquid getting top filters, solid matter after filtration, is filter cake;
Step 2, by quality solid-to-liquid ratio 1:3.5, the sulfuric acid solution being 30% by gained filter cake in above-mentioned steps one and volumetric concentration adds in purification tank, stirs 40 minutes, obtains suspension;
Step 3, gained suspension in above-mentioned steps two is carried out filtration washing, wash to sulfate radical-free ion, moisture is 50%, and gained solid matter is called purification filter cake, is namely carrier, for subsequent use;
Step 4, be 1:25 by quality solid-to-liquid ratio, add in reactor by the carrier prepared by above-mentioned steps three and water, after stirring 8 minutes with the rotating speed of 600r/min, to add volumetric concentration be the pH value of the sulfuric acid solution adjustment mixed solution of 35% is 1; Then stir with the rotating speed of 500r/min and within 10 minutes, add titanium sulfate aqueous solution that concentration is 3mol/L or the aqueous solution of titanyle sulfate that concentration is 3mol/L in backward mixed solution, its addition is 0.05% of mixed liquor volume; Continue to stir with the rotating speed of 600r/min to add the ammonium sulfate solution that concentration is 200g/L in backward mixed solution in 12 minutes, its addition is 0.03% of mixed liquor volume; Add after stirring 15 minutes with the rotating speed of 600r/min again mass concentration be the ammoniacal liquor adjustment ph value of mixture of 15% for 4.5, then continue to stir with the rotating speed of 600r/min and obtain mixture after being incubated 40 minutes;
Step 5, the mixture obtained by above-mentioned steps four is carried out filtering means dehydration, cyclic washing, to sulfate radical-free ion, obtains solid matter, and gained solid matter is dry 4 little of Powdered at 105 DEG C;
Step 6, above-mentioned steps five gained powdered solid substance to be calcined 4 hours at 660 DEG C, after cooling of coming out of the stove, namely obtain nanometer titanic oxide composite photochemical catalyst material.
embodiment 2
A preparation method for nanometer titanic oxide composite photochemical catalyst material, concrete operation step is as follows:
Step one, get natural minerals zeolite powder 1 part, 10 parts, water and the calgon 0.006 part that meso-position radius is less than 9 microns and put into dispersion tank, stir 4 minutes with the rotating speed of 2500r/min, after static 10 minutes, the dispersion liquid getting top filters, solid matter after filtration, is filter cake;
Step 2, by quality solid-to-liquid ratio 1:3.5, the sulfuric acid solution being 30% by gained filter cake in above-mentioned steps one and volumetric concentration adds in purification tank, stirs 40 minutes, obtains suspension;
Step 3, gained suspension in above-mentioned steps two is carried out filtration washing, wash to sulfate radical-free ion, moisture is 50%, and gained solid matter is called purification filter cake, is namely carrier, for subsequent use;
Step 4, be 1:25 by quality solid-to-liquid ratio, add in reactor by the carrier prepared by above-mentioned steps three and water, after stirring 8 minutes with the rotating speed of 600r/min, to add volumetric concentration be the pH value of the sulfuric acid solution adjustment mixed solution of 35% is 2; Then stir with the rotating speed of 500r/min and within 10 minutes, add titanium sulfate aqueous solution that concentration is 3mol/L or the aqueous solution of titanyle sulfate that concentration is 3mol/L in backward mixed solution, its addition is 0.05% of mixed liquor volume; Continue to stir with the rotating speed of 600r/min to add the ammonium sulfate solution that concentration is 200g/L in backward mixed solution in 12 minutes, its addition is 0.03% of mixed liquor volume; Add after stirring 15 minutes with the rotating speed of 600r/min again mass concentration be the ammoniacal liquor adjustment ph value of mixture of 15% for 4.5, then continue to stir with the rotating speed of 600r/min and obtain mixture after being incubated 40 minutes;
Step 5, the mixture obtained by above-mentioned steps four is carried out filtering means dehydration, cyclic washing, to sulfate radical-free ion, obtains solid matter, and gained solid matter is dry 4 little of Powdered at 105 DEG C;
Step 6, above-mentioned steps five gained powdered solid substance to be calcined 4 hours at 700 DEG C, after cooling of coming out of the stove, namely obtain nanometer titanic oxide composite photochemical catalyst material.
embodiment 3
A preparation method for nanometer titanic oxide composite photochemical catalyst material, concrete operation step is as follows:
Step one, get natural minerals sepiolite powder 1 part, 10 parts, water and the calgon 0.006 part that meso-position radius is less than 9 microns and put into dispersion tank, stir 4 minutes with the rotating speed of 2500r/min, after static 10 minutes, the dispersion liquid getting top filters, solid matter after filtration, is filter cake;
Step 2, by quality solid-to-liquid ratio 1:3.5, the sulfuric acid solution being 30% by gained filter cake in above-mentioned steps one and volumetric concentration adds in purification tank, stirs 40 minutes, obtains suspension;
Step 3, gained suspension in above-mentioned steps two is carried out filtration washing, wash to sulfate radical-free ion, moisture is 50%, and gained solid matter is called purification filter cake, is namely carrier, for subsequent use;
Step 4, be 1:25 by quality solid-to-liquid ratio, add in reactor by the carrier prepared by above-mentioned steps three and water, after stirring 8 minutes with the rotating speed of 600r/min, to add volumetric concentration be the pH value of the sulfuric acid solution adjustment mixed solution of 35% is 3; Then stir with the rotating speed of 500r/min and within 10 minutes, add titanium sulfate aqueous solution that concentration is 3mol/L or the aqueous solution of titanyle sulfate that concentration is 3mol/L in backward mixed solution, its addition is 0.05% of mixed liquor volume; Continue to stir with the rotating speed of 600r/min to add the ammonium sulfate solution that concentration is 200g/L in backward mixed solution in 12 minutes, its addition is 0.03% of mixed liquor volume; Add after stirring 15 minutes with the rotating speed of 600r/min again mass concentration be the ammoniacal liquor adjustment ph value of mixture of 15% for 4.5, then continue to stir with the rotating speed of 600r/min and obtain mixture after being incubated 40 minutes;
Step 5, the mixture obtained by above-mentioned steps four is carried out filtering means dehydration, cyclic washing, to sulfate radical-free ion, obtains solid matter, and gained solid matter is dry 4 little of Powdered at 105 DEG C;
Step 6, above-mentioned steps five gained powdered solid substance to be calcined 4 hours at 720 DEG C, after cooling of coming out of the stove, namely obtain nanometer titanic oxide composite photochemical catalyst material.
photocatalysis detects analysis design mothod:
Experiment one:
Weigh the nanometer titanic oxide composite photochemical catalyst material 0.1g prepared by Example in the balance, measuring concentration with graduated cylinder is 100mg/L rhodamine B solution 100mL, successively joins in 500 mL beakers by taken nanometer titanic oxide composite photochemical catalyst material and rhodamine B solution; Beaker is placed on magnetic stirring apparatus and stirs 5 minutes, then irradiate 30 minutes under 360 watts of .250 lie prostrate uviol lamp; Get supernatant in beaker and put into 10000r/min centrifugation in centrifuge, get the stillness of night after centrifugation measures absorbance under spectrophotometer; Calculate the degradation rate of rhodamine B under uviol lamp in 30min according to absorbance, computing formula is as follows:
（1）
In formula (1): K is degradation rate; A
0for the absorbance of the initial stillness of night;
a t for the absorbance of stillness of night sample during reaction time t.The results are shown in Table 1, demonstrating in 30min rhodamine B degradation rate under uviol lamp can reach 96.41%, shows that the nanometer titanic oxide composite photochemical catalyst material prepared by the present invention has higher activity, has higher degradation rate to the harmful substance in air.
Experiment two:
Experimental group method of operating is, the nanometer titanic oxide composite photochemical catalyst material taken prepared by 6g the present embodiment mixes with 24ml water, be coated on the glass plate of four piece of 61 cm × 61 cm, put into the airtight glass box of 1 cubic metre, the culture dish filling 3 μ l formaldehyde is put into case simultaneously; Establish control group simultaneously, four piece of 61 cm × 61 cm is not coated with the glass plate of sample, put into airtight 1 m
3in glass box, the culture dish filling 3 μ l formaldehyde is put into case simultaneously; Then Continuous irradiation 48 h under 30 watts of fluorescent lamps in glass box, after putting into 48 h, adopt phenol reagent method to measure the concentration of two glass box formaldehyde in air, calculate the degradation rate of formaldehyde under fluorescent lamp in 48h according to surveyed concentration of formaldehyde, computational methods are as follows:
Degradation rate=(control group is surveyed concentration of formaldehyde-experimental group and is surveyed concentration of formaldehyde) * 100% of formaldehyde under fluorescent lamp in 48h;
The results are shown in Table 1, demonstrating in 48h formaldehyde degradation rate under fluorescent lamp can reach 81.31%, shows that the nanometer titanic oxide composite photochemical catalyst material prepared by the present invention can by the formaldehyde in effect degraded air.
The photocatalysis of table 1 embodiment sample detects analysis result
Claims (1)
1. a preparation method for nanometer titanic oxide composite photochemical catalyst material, is characterized in that: its concrete operation step is as follows:
Step one, get meso-position radius and be less than the natural minerals zeolite powder of 9 microns or dispersion tank put into by natural minerals sepiolite powder 1 part, 10 parts, water and calgon 0.006 part, 4 minutes are stirred with the rotating speed of 2500r/min, after static 10 minutes, the dispersion liquid getting top filters, solid matter after filtration, is filter cake;
Step 2, by quality solid-to-liquid ratio 1:3.5, the sulfuric acid solution being 30% by gained filter cake in above-mentioned steps one and volumetric concentration adds in purification tank, stirs 40 minutes, obtains suspension;
Step 3, gained suspension in above-mentioned steps two is carried out filtration washing, wash to sulfate radical-free ion, moisture is 50%, and gained solid matter is called purification filter cake, is namely carrier, for subsequent use;
Step 4, be 1:25 by quality solid-to-liquid ratio, add in reactor by the carrier prepared by above-mentioned steps three and water, after stirring 8 minutes with the rotating speed of 600r/min, to add volumetric concentration be the pH value of the sulfuric acid solution adjustment mixed solution of 35% is 1 ~ 3; Then stir with the rotating speed of 500r/min and within 10 minutes, add titanium sulfate aqueous solution that concentration is 3mol/L or the aqueous solution of titanyle sulfate that concentration is 3mol/L in backward mixed solution, its addition is 0.05% of mixed liquor volume; Continue to stir with the rotating speed of 600r/min to add the ammonium sulfate solution that concentration is 200g/L in backward mixed solution in 12 minutes, its addition is 0.03% of mixed liquor volume; Add after stirring 15 minutes with the rotating speed of 600r/min again mass concentration be the ammoniacal liquor adjustment mixed liquor pH value of 15% for 4.5, then continue to stir with the rotating speed of 600r/min and obtain mixture after being incubated 40 minutes;
Step 5, the mixture obtained by above-mentioned steps four is carried out filtering means dehydration, cyclic washing, to sulfate radical-free ion, obtains solid matter, and gained solid matter is dry 4 little of Powdered at 105 DEG C;
Step 6, above-mentioned steps five gained powdered solid substance to be calcined 4 hours at 660 DEG C ~ 720 DEG C, after cooling of coming out of the stove, namely obtain nanometer titanic oxide composite photochemical catalyst material.
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| CN104437343A (en) * | 2014-09-19 | 2015-03-25 | 安徽工程大学 | Modified titanium dioxide and preparation method and application of modified titanium dioxide |
| CN104857931B (en) * | 2015-05-14 | 2017-07-07 | 江苏玖川纳米材料科技有限公司 | A kind of production method of dyeing waste water adsorption-flocculation catalysis material |
| CN104857929A (en) * | 2015-05-14 | 2015-08-26 | 江苏玖力纳米材料科技有限公司 | Vehicle interior VOC adsorption-photocatalytic material production method |
| CN109880464B (en) * | 2019-01-26 | 2021-01-15 | 温州市华汇艺术装饰工程有限公司 | Environment-friendly wall coating for decoration and painting method thereof |
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| CN101804338A (en) * | 2009-05-19 | 2010-08-18 | 王秀宝 | Process for producing nano titanium dioxide/diatomite composite photocatalytic material |
| CN102070151A (en) * | 2010-11-17 | 2011-05-25 | 王泽民 | Method for purifying secondary diatomite |
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| CN101804338A (en) * | 2009-05-19 | 2010-08-18 | 王秀宝 | Process for producing nano titanium dioxide/diatomite composite photocatalytic material |
| CN102070151A (en) * | 2010-11-17 | 2011-05-25 | 王泽民 | Method for purifying secondary diatomite |
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Application publication date: 20130904 Assignee: Luoyang Xinshuo Electric Machinery Equipment Co.,Ltd. Assignor: LUOYANG INSTITUTE OF SCIENCE AND TECHNOLOGY Contract record no.: X2024980001577 Denomination of invention: A nano titanium dioxide composite photocatalytic material and its preparation method Granted publication date: 20150729 License type: Common License Record date: 20240131 |